[Ru6C(CO)17]: a case of organometallic crystal polymorphism

Braga, Dario; Grepioni, Fabrizia; Dyson, Paul J.; Johnson, Brian F. G.; Frediani, Piero; Bianchi, Mario; Piacenti, Franco

doi:10.1039/dt9920002565

Cited by 57 publications

(28 citation statements)

References 12 publications

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“…Ϫ Depending on the reaction time orange-red crystals up to 100 µm length grew in a black powder of Ru particles of nanometer size. This growth behaviour is very similar to the preparation of the carbidocarbonyl Ru 6 C(CO) 17 described by Johnson et al [29] and by Braga et al [30] which could also only be obtained in a moderate yield. Ϫ The purity of the crystals and the Ru/Se ratio of unity was confirmed within an error bar of 3% by using Energy Dispersive X-ray fluorescence.…”

Section: Methodssupporting

confidence: 63%

A New Cubane-Type Ru4(CO)12(µ3-Se)4 Tetramer Tailored for Water Photooxidation Catalysis

Rupp

Nowak

Fiechter

et al. 2001

Eur. J. Inorg. Chem.

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In an effort to tailor a transition metal complex for photoinduced water splitting, a new cubane-like ruthenium chalcogenide tetramer, Ru 4 (CO) 12 (µ 3 -Se) 4 , has been synthesized and structurally characterized by single-crystal X-ray diffraction. The orange-red compound crystallizes in the cubic space group I4 3m. The geometry of the Ru 4 Se 4 units remains undistorted in the cubic symmetry 3m. Such a high symmetry is exceptional among cubane-type cluster compounds. Ruthenium atoms are octahedrally coordinated by three selenium atoms and three CO groups. Ru 4 Se 4 (CO) 12 clusters are linked via van der Waals forces by oxygen atoms which belong to CO ligands of two different cluster units. By stacking of the cluster units along the cubic axes two weakly coupled three-

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Section: Methodssupporting

confidence: 63%

A New Cubane-Type Ru4(CO)12(µ3-Se)4 Tetramer Tailored for Water Photooxidation Catalysis

Rupp

Nowak

Fiechter

et al. 2001

Eur. J. Inorg. Chem.

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“…A similar reaction between 1 and methylcyclopentadiene in toluene gave as the major product the methyl analogue of 2 in 27% yield. When pentamethylcyclopentadiene was used, the pentanuclear vinylidene complex Ru »(/~ 3-CCHPh)(/~4-PPh)(/~-PPh 2)(CO)9 (q-C5 Me 5) (6) was formed in addition to the CsMes analogue of 2, each being obtained in 15 % yield.…”

Section: Resultsmentioning

confidence: 99%

“…Molecular Structure of Rus(~t3-CCHPh)(~t4-PPh)(la-PPh2) (CO)9(q-CsMes) (6) One of the two closely similar independent, pseudo-symmetrically related molecules Of 6 is depicted in Fig. 3 and selected bond parameters are given in TablelII.…”

Section: Resultsmentioning

confidence: 99%

“…Difference map residues and refinement behavior were suggestive of disorder of the ligand peripheral double bond to either side of C(1012); hydrogen atom components were disordered accordingly, any associated carbon disorder being presumed to be encompassed by the thermal envelopes. (6). Pseudo-symmetry is evident in this structure (vide z for corresponding atoms of the two molecules of the asymmetric unit); solvent atoms were refined with constraints on geometry (solvent 1 ) or population [0.797(6) for solvent2].…”

Section: Crystallographymentioning

confidence: 99%

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Cluster Chemsitry. 96. Penta- and hexa-nuclear ruthenium cluster complexes derived from reactions of cyclopentadienes with Ru5(?5-C2PPh2)(?-PPh2)(CO)13

et al. 1994

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“…The interstitial atom can provide electrons from within the cage; an interstitial carbon atom effectively 'replaces' two 2-electron donor ligands whilst adding nothing to the steric crowding around the metal framework. The packing of the carbonyl ligands in Ru6(CO)17C [8] is illustrated in Fig. 3; a related species with an empty Ru6-cavity would have the formula 'Ru6(CO)t9' and would be sterically congested (see below, however, for a related rhenium species).…”

Section: Butterfly Mmentioning

confidence: 99%

Clusters with interstitial atoms from the p-block: How do Wade's rules handle them?

Housecroft

Structural and Electronic Paradigms in Cluster Chemistry

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This article is dedicated to Ken Wade whose thought-provoking undergraduate lectures provided inspiration at a time when Wade's rules were breaking new ground.This article considers the application of Wade's rules of cluster electron counting to low oxidation state transition metal clusters containing interstitial atoms from the p-block. The discussion focuses on the classification of clusters using Wade's rules, and on their successes and failures which can be rationalized in terms of the relationship of a particular metal cluster to a deltahedral [BnHn] 2-anionic prototype cluster. The need to extend the electron counting schemes to the Polyhedral Skeletal Electron Pair Theory (PSEPT) is seen when we consider frameworks such as the trigonal prism which is considered as a 3-connected polyhedron rather than as a hypho-cluster. A square-antiprism Mx-skeleton is ambiguous: such dusters may or may not obey Wade's rules. The application of Wade's rules to condensed polyhedra and the limitations of the rules in this case are considered. Finally, we discuss examples of gold clusters containing interstitial atoms from the p-block and illustrate that the bonding in and the shapes of these clusters are not satisfactorily rationalized by either the Wade or PSEPT approach.

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[Ru6C(CO)17]: a case of organometallic crystal polymorphism

Cited by 57 publications

References 12 publications

A New Cubane-Type Ru4(CO)12(µ3-Se)4 Tetramer Tailored for Water Photooxidation Catalysis

A New Cubane-Type Ru4(CO)12(µ3-Se)4 Tetramer Tailored for Water Photooxidation Catalysis

Cluster Chemsitry. 96. Penta- and hexa-nuclear ruthenium cluster complexes derived from reactions of cyclopentadienes with Ru5(?5-C2PPh2)(?-PPh2)(CO)13

Clusters with interstitial atoms from the p-block: How do Wade's rules handle them?

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